CN114522660A - Novel modified sodium fluoride special adsorbent, preparation and application - Google Patents
Novel modified sodium fluoride special adsorbent, preparation and application Download PDFInfo
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Abstract
The invention provides a novel modified sodium fluoride special adsorbent, and preparation and application thereof. The preparation method comprises the following steps: s1, providing NiCl2·6H2O and porous NaF, and mixing the components according to a mass ratio of 1: 3.0-3.5 to prepare spherical particles; s2, sintering the spherical particles in a vacuum environment at the temperature of 120-130 ℃ and 280-300 ℃ for 10-40 hours and 10-40 hours respectively to form an adsorbent intermediate with a NiCl2-NaF framework, wherein the vacuum degree is less than or equal to 500 pa; s3, treating the adsorbent intermediate with high-purity fluorine-nitrogen mixed gas to finally form the NiF2-novel sodium fluoride adsorbents of NaF framework. The invention provides a novel improvementThe special adsorbent for sodium fluoride can effectively disperse chlorine trifluoride and hydrogen fluoride molecules, the optimal adsorption efficiency of the adsorbent for the sodium fluoride is improved to over 98 percent, and the optimal adsorption efficiency of the adsorbent for the sodium fluoride is reduced to about 3 percent. Furthermore, the novel special modified sodium fluoride adsorbent is simple in manufacturing process, low in production cost, good in economic benefit and capable of being produced industrially.
Description
Technical Field
The invention relates to a novel modified sodium fluoride special adsorbent, preparation and application.
Background
At present, chlorine trifluoride and hydrogen fluoride are easy to associate to form a polymer, and the separation difficulty of the two substances is large. Research shows that the conventional sodium fluoride has stronger stability to chlorine trifluoride and hydrogen fluoride and can adsorb hydrogen fluoride, but the adsorption efficiency of the conventional sodium fluoride to the hydrogen fluoride is lower than 90%, the conventional sodium fluoride has about 10% of adsorption effect to the chlorine fluoride, and the defects of low adsorption efficiency to the hydrogen fluoride, large chlorine trifluoride loss and the like exist.
Disclosure of Invention
The invention provides a novel modified sodium fluoride special adsorbent, preparation and application, and can effectively solve the problems.
The invention is realized by the following steps:
the invention further provides a preparation method of the novel modified sodium fluoride special adsorbent, which comprises the following steps:
s1, providing NiCl2·6H2O and porous NaF, and mixing the components according to a mass ratio of 1: 3.0-3.5 to prepare spherical particles;
s2, sintering the spherical particles in a vacuum environment at the temperature of 120-130 ℃ and 280-300 ℃ for 10-40 hours and 10-40 hours respectively to form the NiF2-a NaF-framed adsorbent intermediate wherein the degree of vacuum is 500pa or less;
s3, treating the adsorbent intermediate by using high-purity fluorine-nitrogen mixed gas.
The invention further provides a novel special modified adsorbent for sodium fluoride, which has NiF2A NaF framework and a BET specific surface area of 2m or more2·g-1Pore volume is more than or equal to 0.00015cm3·g-1。
The invention further provides a novel special modified sodium fluoride adsorbent, which is obtained by the method.
The invention further provides an application of the novel special modified sodium fluoride adsorbent, and the novel special modified sodium fluoride adsorbent is used for separating chlorine trifluoride from hydrogen fluoride.
The invention has the beneficial effects that: the invention aims at the association of chlorine trifluoride and hydrogen fluoride to develop NiF2The novel modified sodium fluoride special adsorbent with the NaF configuration and the preparation method thereof remove hydrogen fluoride impurities by dispersing chlorine trifluoride and hydrogen fluoride, improve the purity of chlorine trifluoride and meet the application requirement of chlorine trifluoride. The novel special modified adsorbent for sodium fluoride provided by the invention can effectively disperse chlorine trifluoride and hydrogen fluoride molecules, the optimal adsorption efficiency of the adsorbent for hydrogen fluoride is improved to more than 98%, and the optimal adsorption efficiency of the adsorbent for chlorine trifluoride is reduced to about 3%. In addition, the novel modified sodium fluoride special adsorbent can keep high activity and high adsorbability under various working conditions. Furthermore, the novel special modified sodium fluoride adsorbent is simple in manufacturing process, low in production cost, good in economic benefit and capable of being produced industrially.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are required to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
FIG. 1 is a scanning electron micrograph of conventional sodium fluoride.
Fig. 2 is a scanning electron micrograph of the novel modified sodium fluoride special adsorbent provided in the embodiment of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions of the embodiments of the present invention will be described clearly and completely with reference to the accompanying drawings of the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all embodiments of the present invention. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention. Thus, the following detailed description of the embodiments of the present invention, presented in the figures, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
In the description of the present invention, the terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or to imply that the number of technical features indicated is significant. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of the present invention, "a plurality" means two or more unless specifically defined otherwise.
The embodiment of the invention provides a preparation method of a novel special modified sodium fluoride adsorbent, which comprises the following steps:
s1, providing NiCl2·6H2O and porous NaF, and mixing the components according to a mass ratio of 1: 3.0-3.5 to prepare spherical particles;
s2, sintering the spherical particles in a vacuum environment at the temperature of 120-130 ℃ and 280-300 ℃ for 10-40 hours and 10-40 hours respectively to form the NiF-containing particles2-a NaF-framed adsorbent intermediate wherein the degree of vacuum is 500pa or less;
s3, treating the adsorbent intermediate by using high-purity fluorine-nitrogen mixed gas.
As a further improvement, in step S1, the test proves that NiCl2·6H2The proportion of O and porous NaF is controlled to be beneficial to NiCl2NiF formed by fluorination2Fully combined with NaFThe adsorption efficiency of chlorine trifluoride is reduced to the maximum. Therefore, preferably, NiCl is added2·6H2O and porous NaF according to a mass ratio of 1: 3.1 to 3.3, and making into spherical particles. In one embodiment, NiCl is added2·6H2O and porous NaF according to a mass ratio of 1: the ratio of 3.2 was made into spherical particles.
The porous NaF can be prepared by the following steps:
s11, adding NaHF2Vacuum treating to remove at least part of hydrogen atoms from NaHF2The molecules escape to form loose and porous substances with the property of sodium fluoride; wherein the drying temperature is 200-. In one embodiment, the drying temperature is about 205 ℃, the drying time is about 24 hours, and the vacuum degree is about 100 pa.
In a further improvement, in step S1, the spherical particles have a particle size of 5 to 8 mm. The particle size facilitates packing of the adsorption column to provide a greater porosity. As a further improvement, the NiCl2Can be further processed to form polyfluoro substances and form nickel fluoride with higher fluorine content.
As a further improvement, in step S2, sintering is performed in a step-like manner to prevent the temperature from rising too high, which causes spherical particles to crack, thereby increasing the sintering yield, and the specific surface area and pore volume of the sintered adsorbent particles are increased several times. Further, NiCl may be further sintered by the step-form sintering2·6H2Water molecules of O and part of NaHF with further H atoms2To form a loose porous grain structure. In one embodiment, the spherical particles are sintered in vacuum at 125 deg.C and 290 deg.C for 24 hr and 24 hr respectively, and the vacuum degree is about 100pa, so that the final BET specific surface area can reach 4.0756m2·g-1The pore volume can reach 0.000301cm3·g-1. In another embodiment, the spherical particles are sintered in a vacuum environment at 130 deg.C, 280 deg.C for 24 hours and24 hours and the vacuum degree is about 100pa, so that the final BET specific surface area can reach 4.8995m2·g-1The pore volume can reach 0.000356cm3·g-1. In another embodiment, the spherical particles are sintered in vacuum environment at 120 deg.C and 300 deg.C for 24 hr and 24 hr respectively, and the vacuum degree is about 100pa, so that the final BET specific surface area can reach 3.9781m2·g-1The pore volume can reach 0.000293cm3·g-1。
As a further improvement, in step S3, the use of the high-purity mixed gas of fluorine and nitrogen has an effect of fluorinating nickel chloride by the fluorine gas to form nickel fluoride. The nickel fluoride with high fluorine content is introduced into the sodium fluoride (one nickel atom is combined with two fluorine atoms in each molecule), and through the combination action of the sodium fluoride molecules and the nickel difluoride molecules, multi-fluorine radical 'molecules' similar to chlorine trifluoride in spatial configuration are formed, and the bond length and the bond angle between the molecules of the chlorine trifluoride and the molecules of the sodium fluoride are twisted to a certain extent, so that the aim of dispersing the molecules of the sodium fluoride and the chlorine trifluoride is fulfilled. When the molecules of the polyfluoro group act with hydrogen fluoride molecules, intermolecular weak acting force is easier to form, the temperature of a mixture system is controlled, the formation of high polymers of the hydrogen fluoride molecules is reduced, meanwhile, the bimolecular association of chlorine trifluoride molecules is also reduced, and the repulsive force between the molecules with higher activity and the molecules of the modified sodium fluoride is synchronously increased, so that the aims of reducing the adsorption of chlorine trifluoride and improving the adsorption of hydrogen fluoride by the modified sodium fluoride are fulfilled. The nitrogen gas acts to dilute the fluorine gas, preventing the danger due to the strong activity of the fluorine gas. Experiments have shown that when the fluorine gas concentration is too low, the activity is insufficient, and when the concentration is high, danger is liable to occur. Therefore, preferably, the high-purity fluorine-nitrogen mixed gas comprises 5-15% of F by volume2And N in an amount of 85 to 95% by volume2. In one embodiment, the high purity fluoroazine mixture includes about 10% F by volume2And 90% by volume of N2。
As a further improvement, in step S3, the step of treating the adsorbent intermediate with a high-purity fluorine-nitrogen mixed gas includes:
and fluorinating the adsorbent intermediate for 24-72 hours by using high-purity fluorine-nitrogen mixed gas. In one embodiment, the adsorbent intermediate is fluorinated with high purity fluorine nitrogen gas for 48 hours, and after the fluorination is completed, the high purity fluorine nitrogen gas is removed by purging with nitrogen.
The invention further provides a novel special modified adsorbent for sodium fluoride, which has NiF2-NaF framework and BET specific surface area of 2m or more2·g-1Pore volume is more than or equal to 0.00015cm3·g-1. In one embodiment, the BET specific surface area of the novel special modified sodium fluoride adsorbent can reach 4.8995m2·g-1The pore volume can reach 0.000356cm3·g-1。
Referring to fig. 1-2, at present, conventional sodium fluoride is in a dense crystal arrangement, has a small specific surface area, and is not favorable for efficient adsorption of hydrogen fluoride (the BET specific surface area can only reach 0.6591 m)2·g-1The pore volume can only reach 0.000054cm3·g-1). The modified novel special modified sodium fluoride adsorbent has a sheet structure and a large specific surface area, the number of holes is increased compared with that of conventional sodium fluoride, and the adsorption efficiency of hydrogen fluoride can be effectively improved.
The embodiment of the invention further provides an application of the novel special modified sodium fluoride adsorbent, and the novel special modified sodium fluoride adsorbent is used for separating chlorine trifluoride and hydrogen fluoride.
In the present invention, the separation of chlorine trifluoride from hydrogen fluoride was subjected to an orthogonal test under the following process conditions:
TABLE 1 orthogonal test factors
Table 2 shows the results of the orthogonal test
From the above table 2, it can be seen that the novel modified sodium fluoride special adsorbent provided by the present invention can effectively disperse chlorine trifluoride and hydrogen fluoride molecules, the optimal adsorption efficiency for hydrogen fluoride is increased to above 98%, and the optimal adsorption efficiency for chlorine trifluoride is reduced to about 3%. In addition, the novel modified sodium fluoride special adsorbent can keep high activity and high adsorbability under various working conditions. Furthermore, the novel special modified sodium fluoride adsorbent is simple in manufacturing process, low in production cost, good in economic benefit and capable of being produced industrially. Finally, the adsorbent has long service life, and experiments prove that the optimum adsorption efficiency of the hydrogen fluoride can be kept to about 98 percent and the optimum adsorption efficiency of the chlorine trifluoride can be kept to about 3 percent after the adsorbent is repeatedly used for 100 times.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (9)
1. A preparation method of a novel modified sodium fluoride special adsorbent is characterized by comprising the following steps:
s1, providing NiCl2·6H2O and porous NaF, and mixing the components according to a mass ratio of 1: 3.0-3.5 to prepare spherical particles;
s2, sintering the spherical particles in a vacuum environment at the temperature of 120-130 ℃ and 280-300 ℃ for 10-40 hours and 10-40 hours respectively to form NiCl2-a NaF-structured adsorbent intermediate wherein the degree of vacuum is 500pa or less;
s3, treating the adsorbent intermediate by using high-purity fluorine-nitrogen mixed gas.
2. The method for preparing the novel modified adsorbent dedicated to sodium fluoride according to claim 1, wherein in step S1, the step of preparing the porous NaF comprises:
s11, adding NaHF2Vacuum drying to form loose and porous sodium fluoride matter; wherein the drying temperature is 200-210 ℃, the drying time is 20-30 h, and the vacuum degree is less than or equal to 500 pa.
3. The method for preparing the novel modified adsorbent dedicated to sodium fluoride according to claim 1, wherein in step S1, the spherical particles have a particle size of 5 to 8 mm.
4. The method for preparing the novel modified sodium fluoride special-purpose adsorbent as claimed in claim 1, wherein in step S3, the high-purity mixed gas of fluorine and nitrogen comprises 5-15% by volume of F2And N in a volume content of 85-95%2。
5. The method for preparing the novel modified adsorbent dedicated to sodium fluoride according to claim 1, wherein in step S3, the step of treating the adsorbent intermediate with the high-purity fluorine-nitrogen mixed gas comprises:
and fluorinating the adsorbent intermediate for 24-72 hours by using high-purity fluorine-nitrogen mixed gas.
6. The novel special modified adsorbent for sodium fluoride is characterized by comprising NiF2A NaF framework and a BET specific surface area of 2m or more2·g-1Pore volume is more than or equal to 0.00015cm3·g-1。
7. A novel modified adsorbent dedicated to sodium fluoride, which is obtained by the method according to any one of claims 1 to 5.
8. The use of the novel modified adsorbent dedicated to sodium fluoride as claimed in claim 6 or 7, wherein the novel modified adsorbent dedicated to sodium fluoride is used for separating chlorine trifluoride from hydrogen fluoride.
9. The use of the novel modified sodium fluoride-specific adsorbent as claimed in claim 8, wherein the separation conditions comprise: the temperature is 80-100 ℃, the flow rate is 0.2-1L/min, and the pressure is 0.6-1 MPa.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115558149A (en) * | 2022-09-28 | 2023-01-03 | 江苏龙灯博士摩包装材料有限公司 | Efficient fluorination processing technology for fluorination barrel |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115558149A (en) * | 2022-09-28 | 2023-01-03 | 江苏龙灯博士摩包装材料有限公司 | Efficient fluorination processing technology for fluorination barrel |
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